RU2696313C2 - Oxidation retardation in food systems using lipid-soluble tea catechines - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: invention is intended for usage in meat industry. Method for slowing down oxidation of food products having a boundary line of lipid and aqueous phases is characterized by that it includes a step of adding catechins of green tea esterified to complex palmityl esters in amount of 250–1000 ppm. Catechins of green tea, esterified to complex palmitol esters, are introduced into food product together with antioxidant compounds by way of mixing. Food products are selected from a group consisting of food emulsions, meat products, as well as products of cereals and crushed grain with low fat content, wherein food emulsions are selected from a group consisting of mayonnaise, margarine and dressing for salad. Lipid-soluble tea catechines are suitable for use in decelerating undesirable colour changes and in prolonging oxidative stability of meat products, food emulsions and extruded food products, as well as in slowing down the formation of oxidation products in margarine and salad dressings.

EFFECT: composition is effective while maintaining desired red colour of meat products, as well as during inhibition of formation of oxidative by-products, compared to non-processed meat products, while maintaining low levels of oxidative products in food emulsions and maintaining low levels of secondary oxidative products and acceptable organoleptic profiles for extruded food products.

10 cl, 9 dwg, 19 tbl

Description

This application claims the priority of United States Patent Application 62/043690, filed August 29, 2014, which is incorporated herein by reference in its entirety.

State of the art

The present invention generally relates to the use of catechins extracted from tea, which are esterified to produce lipid-soluble esters of tea catechins, which are found to be effective in slowing down oxidation in food products.

While water-soluble catechins of green tea are widely used and act as antioxidants, their use is limited in high-fat food matrices. The active compounds in lipid-soluble tea catechins (LSC), in catechin esters, have functional catechin residues, which malfunction excellent free radical scavengers, serving as antioxidants. The oil solubility of catechin esters is improved by adding long alkyl chains from the palmityl functional group, making them thus more usable and effective for higher fat matrices. One of the advantages of LSC is a lower profile of flavoring substances, which makes it possible to use them at higher processing levels than for certain other botanical extracts, such as rosemary extract, with increased efficiency.

In addition to this, although LSC is lipid soluble, it also serves as an effective ingredient in protecting food emulsions and meat, since LSC is believed to be present at the interface of the lipid and aqueous phases present in these products. Since the oxidation rate is the highest at the interface, and the LSC is localized near it, it could maximize its function in stabilizing fats and slow down the formation of oxidation by-products.

SUMMARY OF THE INVENTION

The present invention describes the use of lipid-soluble tea catechins in slowing down unwanted color changes and prolonging the oxidative stability of meat products, food emulsions and extruded food products. This composition, as shown, is effective in maintaining the desired red color of meat products, as well as in slowing the formation of oxidative by-products compared to untreated meat products, slowing down the formation of oxidative products in food emulsions and maintaining acceptable organoleptic profiles in extruded food products.

LSCs are used in distillate fats and oils, in some places, since lipid-soluble tea catechins could protect lipids from oxidation. However, in the present invention, it is new that LSCs are used in food emulsions, meat products, and low-fat cereal and crushed grain products. Due to the molecular structure of LSC, it would be present at the interface between lipids and the aqueous phase, which would maximize its antioxidant function. This hypothesis is supported by the data presented in the present invention.

The obvious use of LSC is its use in distillate fats and oils. It is not obvious that LSC has the best antioxidant functions in meat products, food emulsions, and low fat extruded foods. LSC can be used at various levels of processing and as a combined product with other ingredients, including rosemary extract and mixed tocopherols.

The aim of the present invention is to provide a method for slowing down oxidation in food products having a lipid and aqueous phase interface, comprising the step of mixing an effective amount of tea catechins esterified to palmityl esters.

Brief Description of the Figures

Figure 1 is a graph of the dependence of the values of the peroxide number (meq / kg of fat) versus time in mayonnaise with the mentioned types of processing.

Figure 2 is a graph of the number of alkenals (nmol / ml) versus time in mayonnaise for the treatment in question.

Figure 3 is a graph of the dependence of the values of the peroxide number (meq / kg fat) in products from cereals or from crushed grain, which are stored at 40 ° C; error values represent the standard deviation for two downloads.

Figure 4 is a graph of changes in the content of hexanal (ppm) in products from cereals or from crushed grain, which are stored at 40 ° C; error values represent the standard deviation for two downloads.

Figure 5 is a graph of the change in peroxide number (meq / kg fat) for margarine during storage at 35 ° C.

6 is a graph of the p-anisidine number change for margarine during storage at 35 ° C.

Fig. 7 is a graph of alkenale content (nmol / ml) for farm salad dressing during accelerated storage.

Fig. 8 is a graph of the change in peroxide value (meq / kg fat) for a farm salad dressing during accelerated storage.

Fig.9 is a graph of the change in the volume fraction of the phase of the emulsion, under the influence of adding emulsifiers such as oil in water, including span 80, TGDO and LSC.

Detailed Description of Preferred Embodiments

Definitions

Before explaining the various embodiments of the present invention, it is necessary to understand that the present invention is not limited in its application to the details of the structure and arrangement of the components described in the following description. Other embodiments may be embodied or implemented in various ways. It is also necessary to understand that the phraseology and terminology used in the present invention is intended for description purposes and should not be construed as limiting.

In the present description, various publications, patents and published patent descriptions are mentioned. Where appropriate, descriptions of these publications, patents, and published patent descriptions are hereby incorporated by reference into the present description in their entirety for a more complete description of the prior art.

To facilitate understanding of the description, the following definitions are offered:

The number of compositions of the present invention to be used in specific applications of the present invention can easily be determined by one skilled in the art as a function of the nature of the composition used and / or the desired effect. Typically, this amount can be in the range between 0.01% and 2% by weight with respect to the total weight of the food product that is processed, in particular in the range between 0.2% and 1.5% by weight, preferably in the range between 0, 5% and 1% of the mass, and particularly preferably in the range between 0.6% and 0.9% of the mass.

In preferred embodiments of the present invention, an effective amount of a mixture of lipid-soluble catechins is in the range of 10 ppm. up to 5000 ppm masses from products that are processed, and include all values within these limits, including, for example, without limitation or exclusion, 0.02%, 0.104%, 0.132%, 0.217%, 0.336%, 0.489%, 1.377% and 1.990%. Formulating in another way, in preferred embodiments of the present invention, the dosage can be any ʺabc0ʺ ppm, where it is selected from the numbers 0, 1, 2, 3, 4 and 5, and b and c are each individually selected from the numbers 0 , 1, 2, 3, 4, 5, 6, 7, 8, and 9, with the exception that c cannot be less than 1 if both a and b are 0.

When ranges of values are used in the present description, only the endpoints of these ranges are provided so as to exclude too long a wording and describe each and any value included in this range. You can select any appropriate intermediate value and range between the end points. As an example, if a range between 0.1 and 1.0 is mentioned, all intermediate values (e.g., 0.2, 0.3, 6.3, 0.815, and so on) are included, as are all intermediate ranges ( e.g. 0.2-0.5, 0.54-0.913, and so on).

As used in the present invention, the singular includes the reference to the plural, unless the context dictates clearly otherwise. So, for example, the mention of “factor” refers to one or more factors, and the mention of “processing method” includes the mention of equivalent stages and methods known to specialists in this field, and so on.

The term "antioxidant", as used in the present invention, refers to a composition that prevents or slows down the oxidation of food products. Antioxidants are generally classified as either synthetic or natural. Antioxidants include, but are not limited to, BHA, BHT, tert- butylhydroquinone (TBHQ), gallates, ascorbic acid, erythorbic acid, ascorbyl palmitate, tocopherols, tocotrienols, carotenoids, anthocyanins, polyphenols, citric acid, etin, etin, lectin, etin, eta, polyphosphates, tartaric acid, trihydroxybutyrophenone, thiodipropionic acid and dilauryl and distearyl esters.

The term "effective amount" or "effective amount" refers to the effective amount, at such dosages and for such a period of time that are necessary to achieve the desired result. The effective amount of the compositions of the present invention may vary depending on factors such as the composition or preparation of the product that is processed using the methods and / or compositions of the present invention.

The term "emulsion" refers to a mixture prepared from two mutually insoluble components. Mixtures with a homogeneous macroscopic appearance can be generated from these components by appropriate selection of mixing conditions and manipulation of the mixing conditions. The most common type of emulsions are emulsions that use an aqueous component and a lipophilic component and which are often referred to in the art as oil-in-water and water-in-oil emulsions. In oil-in-water emulsions, the lipophilic phase is dispersed in the aqueous phase, while in water-in-oil emulsions, the aqueous phase is dispersed in the lipophilic phase.

The term “catechins” refers to polyphenolic compounds present in the leaves of Camellia sinensis . Green tea polyphenols include, but are not limited to (-) - epicatechin (EC), (-) - epigallocatechin (EGC), (-) - epicatechin-3-gallate (ECG), (-) - epigallocatechin-3-gallate (EGCG), proanthocyanides, their enantiomers, their epimers, their isomers, their combinations and their prodrugs. "Lipid-soluble tea catechins" refers to green tea polyphenols esterified so that they have one or more hydrocarbon chains, for example, C1-C30. Lipid-soluble tea catechins specifically include the products of the esterification reaction of tea catechins with saturated and unsaturated C1-C30 fatty acids.

"Lipid-soluble" as used in the present invention refers to substances that have a solubility equal to or greater than 5 g / 100 ml in a hydrophobic liquid, such as castor oil.

"Margarine", as used in the present invention, refers to a simulation paste that mimics a product based on milk fat containing vegetable oil and water and consisting of an emulsion of water in fat.

“Oxidative or oxidative stability”, as used in the present invention, is a measure of the oxidation stability of a food product.

“Water-soluble” as used in the present invention refers to substances that have a solubility equal to or greater than 5 g / 100 ml of water.

EXAMPLE 1 - Meat

The shelf life of packaged meat products is limited by microbial contamination and oxidative rancidity. Lipid oxidation is responsible for unwanted odor and color changes, and it is the main cause of spoilage of frozen meat products. Natural extracts derived from plant materials have been shown to slow down these oxidative changes. A finely divided pork protein product (FTP) is obtained by pressing / grinding pork shoulder bones to extract protein from the bones. The FTP is then heated to about 50 ° F (8 ° C) after compression, placed in 50 lb (22.5 kg) boxes, granulated and sent to a freezer with heavy air movement. Due to the difficult processing parameters, at present, the shelf life in packed form is 20 days, frozen, and the desired shelf life in packed form for the consumer is 30-45 days, if we consider the use of this ingredient in pepperoni (10-15 % of the meat composition). The gold standard would be 45 days. The purpose of this study is to evaluate the effect of various treatments, including FORTIUM ^® _brand R30 Liquid (rosemary extract / sunflower oil), FORTIUM ^® _brand RGTWS 1200 Liquid (rosemary / green tea extract / Polysorbate 80 / glycerol monooleate / propylene glycol), FORTIUM ^® _brand R -WS 20 Liquid (rosemary extract / Polysorbate 80 / glycerol monooleate / propylene glycol) and GT-FORT 101 SF Liquid (lipid-soluble tea catechins / sunflower oil) (all supplied from Kemin Industries, Inc., Des Moines, Iowa) for quality parameters FTP

Materials and methods

Materials Frozen FTP is provided by the consumer. Products used in FTP processing are retrieved locally. The following preparations are prepared for processing 1) without treatment, 2) FORTIUM ^® _brand R30 0.1% (lot 1403102012) (R30), 3) FORTIUM ^® _brand RGTWS 1200 0.25% (lot 1309102599) (RGT-WS 1200), 4) FORTIUM ^® _brand R-WS 20 0.25% (lot 1402109597) (R-WS 20) and 5) GT-FORT ^TM 101 SF Liquid 0.3% (lot 20140326-01). All types of processing are given in relation to the total weight of pork.

Mixing Instructions.Mixer Kitchenaid^® (325 watts, St. Joseph, MI) and stainless steel cups were placed in a portable refrigerator (37 ° F (2 ° C)) for cooling. FTP makes it possible to thaw at a cooling temperature (37 ° F (2 ° C)) before being divided in portions for 5 types of processing. Weigh FTP (900 grams) for each download. Fifty grams are removed and the remaining 850 grams are placed in chilled mixer cups. Preparations for processing are mixed manually in the set aside 50 grams of FTP (approximately 2 minutes). The cup is placed on the base of the mixer, and setting 3 is set for stirring speed, 50 grams of the processed FTP is added to the remaining 850 grams and mixing is carried out for 2-3 minutes using a paddle mixer. After stirring, the chilled FTP-treated cup was placed in a Chilzstone refrigeration tray (Castle Rock, CO), and 30-40 gram samples were placed in 18oz (500 g) Whirl-Pak ™ bags (Fisher Scientific catalog # 018125B). When each bag is filled, it is smoothed, flattened, sealed and placed in another Chilzstone for freezing. Samples are stored at 1 ° F (-14 ° C) in a cardboard box for freezing tests and at 36 ° F (1 ° C) for cooling studies.

Chemical and physical analyzes . Treated FTP is evaluated for the presence of oxidative by-products (malonaldehydes) using the reactive substance thiobarbituric acid (TBARS) and color numbers L * a * b * (Hunter Colorimeter).

Stability analysis . The stability study on frozen samples, for TBARS, is carried out twice a week for the first 2 weeks, then, the study is carried out every 7 days. Color analysis is carried out twice a week for 4 weeks, then every 7 days for 63 days in total. Color analysis is carried out on chilled samples on the day of removal from the freezer (initial) and after 4 days of storage in a refrigerated state.

results

Chilled storage. The results for analyzes with TBARS are shown in Table 1, with the exception of days 14 and 21, the untreated sample has the highest content of oxidative by-products.

Table 1. Results for FTP with TBARS (mg / kg) (days)

Treatment Initial value 3 7 ten 14 21 28 35 42 49 57 64 Raw 1.40 1.43 1.68 1.36 1.29 2,39 1.93 1.79 3.17 4.13 2.91 3.38 R30 0.1% 1.09 1.14 1.40 1.14 1.12 3.07 1.23 0.90 1,11 1.26 1.00 0.46 RGT-WS1200 0.25% 1.10 1.01 1.05 1,04 1,53 1.88 1.25 0.92 1.14 1.22 0.87 0.44 R-WS20 0.25% 1.01 1.17 1,08 1.15 1.68 2.16 1.14 0.94 1,08 1.29 1.06 0.50 GT-FORT 101 SF 0.3% 1,04 1,08 1.20 1.21 1.92 1.30 1.43 1.47 1.30 1.32 1.35 0.39

The color analysis results are shown in Tables 2, 3, and 4. The L * values indicate the lightness / darkness of the sample (0 = black, 100 = white), the a * values indicate the red / green ratio (+ indicates more red, indicates more green) and b * values indicate the yellow / blue ratio (+ indicates more yellow, indicates more blue). Hunter a * values are considered the most relevant for this matrix. The percent changes from the initial value to 63 are: for the untreated sample - (-20.88), for R30 - (-4.08), for R-WS 20 - (-4.75), for RGTWS 1200 (+1 , 14) and for LSC - (-14.75).

Table 2. L * Values for FTP

Raw R30 R-WS 20 RGT-WS 1200 GT-FORT 101 SF Initial value 49.92 46.49 47.74 47.15 43.57 Day 3 49.08 42.95 44.58 43.09 44.52 Day 7 49.46 50.01 49.29 49.17 44.07 Day 10 47.31 48.22 50.70 48.79 47.22 Day 14 50.67 50.01 49.29 49.17 44.07 Day 17 45.63 41.65 43.17 42.95 42.48 Day 21 47.95 48.14 45.54 47.81 44.80 Day 24 48,43 44.40 44,99 46.92 44.93 Day 28 47.98 41.44 41.72 42.07 41.22 Day 35 45.27 47.80 47.98 44.35 44.77 Day 42 45.66 45.60 43.96 45.66 44.70 Day 49 48.90 43.84 40.61 40,45 39.06 Day 57 47.19 41.10 46.56 42.79 40.53 Day 63 42.50 42.02 41.32 42.40 42.53

Table 3. A * Values for FTP

Raw R30 R-WS 20 RGT-WS 1200 GT-FORT 101 SF Initial
value 35.81 31.59 33.25 30.68 34.23 Day 3 33,20 35.56 37.22 35.45 36,42 Day 7 34.79 30.69 31.94 31.34 35.05 Day 10 37.39 32,48 30.04 29.63 32.95 Day 14 34.36 30.69 31.94 31.34 35.05 Day 17 34.80 35.10 33.66 34.45 35.04 Day 21 33.05 29.43 30.93 28.76 31,50 Day 24 33.32 33.30 31.66 29.36 33.55 Day 28 28.37 29.14 30.27 28.27 29.16 Day 35 28.38 28.62 27.48 28.67 32.14 Day 42 33.87 28.23 30.29 27.86 31.26 Day 49 30.36 29.39 32.77 30.89 31.79 Day 57 29.08 32.65 26.15 31.32 34.63 Day 63 28.33 30.30 31.67 31.03 29.18

Table 4. b * Values for FTP

Raw R30 R-WS 20 RGT-WS 1200 GT-FORT 101 SF Initial
value 30.41 27.01 25.98 23.75 26.11 Day 3 26.98 30.17 30.09 26.75 30.67 Day 7 27.71 24.94 25.07 24.38 29.08 Day 10 30.61 26.16 23.44 22.98 26.04 Day 14 27.48 24.94 25.07 24.38 29.08 Day 17 30.37 30.80 29.41 28.78 31.48 Day 21 27.93 25.08 24.24 21.65 26.33 Day 24 26.95 24.77 25.70 24.80 28.30 Day 28 22.04 21.08 21.35 18.93 19.93 Day 35 25.79 23.71 22.28 24.05 26.37 Day 42 28.34 23.77 25.30 20.74 27.42 Day 49 27.48 24.73 28.69 25.54 25.56 Day 57 22.96 27.08 20.48 26.06 29.91 Day 63 26.21 28.11 27.09 27.40 25.55

Chilled storage . The results according to the Hunter Colorimeter for refrigerated storage are shown in Tables 5, 6 and 7. All samples have higher L * values and lower a * values on day 4, compared with the initial study, this shows that they become brighter and less red. On day 7, samples deteriorate, so further evaluations are not carried out.

Table 5. L * value for FTP

Raw R30 R-WS 20 RGT-WS 1200 GT-FORT 101 SF Initial value * 42.50 42.02 41.32 42.40 42.53 Day 4 47.74 45.37 46.83 46.66 46.05

* initial values are obtained from day 63 of storage in a refrigerated state

Table 6. A * value for FTP

Raw R30 R-WS 20 RGT-WS 1200 GT-FORT 101 SF Initial value 28.33 30.30 31.67 31.03 29.18 Day 4 8.78 28.21 24.32 23.59 24.93

Table 7. Valueb *for FTP

Raw R30 R-WS 20 RGT-WS 1200 GT-FORT 101 SF Initial value 26.21 28.11 27.09 27.40 25.55 Day 4 18.34 29.50 24.36 23.61 26.27

A visual assessment shows that the untreated sample loses its desired red color compared to all processed samples.

Discussion

For storage in the frozen state from day 28 onwards, the untreated sample has the highest TBARS value compared to all processed samples, for which it is significantly lower. In the last frozen analysis with TBARS (day 64), all processed samples have similar results with respect to oxidative by-products, which shows that all treatments are effective and have similar efficacy in slowing the occurrence of oxidative rancidity compared to an untreated sample. Analysis according to Hunter Colorimeter shows that the untreated sample has the highest decrease in a * values from the initial value to day 63 when stored in the frozen state, this shows that all types of processing support more desirable red color and do it more efficiently than the untreated sample. For refrigerated storage, there are obvious visual differences between untreated and processed samples, this shows that all types of processing are effective in maintaining a more desirable red color.

These results show that using FORTIUM® _brand R30, FORTIUM® _brand R-WS 20, FORTIUM® _brand RGTWS 1200 or LSC in FTP slows down the formation of oxidative by-products and maintains a more desirable color, resulting in an extended shelf life of packaged .

EXAMPLE 2 - Mayonnaise

The mayonnaise is prepared at home and treated with FORTIUM® _brand R30 (rosemary extract / sunflower oil) (R30), lipid-soluble catechins (LSC) and ethylenediaminetetraacetic acid (EDTA) (as a positive control), and also use it as an untreated negative control and stored under environmental conditions. The oxidation of mayonnaise is monitored by examining the peroxide number (PV) and the number of alkenals on a monthly basis for 4 months. The results show that mayonnaise, both LSC-treated and EDTA-treated, results in the lowest amount of oxidation products during the entire study period, which indicates that LSC may be suitable as a substitute for EDTA in mayonnaise.

Materials and methods

Making mayonnaise.For cooking mayonnaise (see Table 8 and Table 9), egg yolks are first beaten in a KitchenAid mixer^® (Heavy Duty) using a whipping wire nozzle for 30 seconds at setting # 2. Add salt and mustard, and mix everything for an additional 30 seconds when setting # 4. The side walls are cleaned with a spoon 3 times. Then add water and carry out stirring for 30 seconds when setting # 2. The side walls are cleaned again. The mixture is then stirred for an additional 30 seconds at setting # 4. Soybean oil is added very slowly with stirring, at setting # 4, in small portions (especially at the beginning, when only a few milligrams of oil are added, and allow them to be absorbed into the mixture before adding more). Toward the end, the oil is added in a thin stream. After adding all the oil, add vinegar for 30 seconds with stirring at setting # 2. The resulting mixture is stirred for an additional 30 seconds, alternately, when setting # 2 and setting # 4. The total mixing time is 5-10 minutes for each load.

The use of antioxidants . Three processed mayonnaise batches are prepared, and one untreated control is prepared for comparison. Each download contains 1,500 g of mayonnaise. Types of processing include: A. 500 ppm R30 (0.7501 g is added to the oil); B. 250 ppm LSC (0.3752 g added to the oil); C. 75 ppm EDTA (0.1131 g added to water). The dosage of EDTA is the upper limit allowed that may be added to mayonnaise in the USA.

Sampling and research . Eight 100 g samples are placed in separate 125 ml plastic bottles for each charge. Bottles are stored on an open shelf in the laboratory at ambient temperature for 4 months. At the end of each month, one bottle from each charge is placed in a freezer at -20 ° C overnight, and thawed the next day to room temperature to break the emulsion. If the emulsion is still stable after freezing / thawing, the emulsion sample is transferred to a centrifuge tube and centrifuged at 10,000 rpm for 10 minutes. After the destruction of the emulsion, there are two liquid phases. The resulting oil phase (top layer) is used for analysis of the peroxide number (PV) and the number of alkenals.

Analysis of PV and the number of alkenals.For PV / alkenale analysis, 1.00 ± 0.01 g of oil is transferred to a 15 ml centrifuge tube (Thermo Scientific, Catalog # 362694). Research is carried out according to established methods. The reagents used for the analysis are shown in Table 10. Briefly, 9.0 ml of the preparation reagent (obtained by adding 3.87 g of butylated hydroxytoluene in 4 L of isopropanol) is added to each tube. The sample was mixed in a vortex mixer (Fisher Digital Vortex Mixer, Catalog # 120123017) for 1 minute, and then centrifuged at 4000 rpm for 5 minutes (Sorvall ST16 centrifuge, Thermal Scientific). For analysis, a supernatant is used.

For PV analysis (which measures the initial oxidation products), 100 μl of the supernatant is added to a glass test tube (12 × 75 mm). One aliquot (3.5 ml) of the preparation reagent is added. Then it is mixed with a solution of 400 μl of xylenol orange indicator solution. The mixture is briefly mixed in a vortex mixer and placed in a shaker. Exactly 5 minutes after this, the sample was recorded using a 570 nm / 690 nm filter on a MicroChem II Spectrophotometer to obtain PV by the FOX II method. For analysis of alkenals in mayonnaise (which measures secondary oxidation products), 150 μl of the supernatant is added to a glass test tube (12 × 75 mm). Distribute one aliquot of each reagent from reagent A and reagent B AlkalSafe (MP Biomedicals). Samples were mixed in a vortex mixer and allowed to stand for 20 minutes, then recorded using a 550 nm / 690 nm filter on a MicroChem II Spectrophotometer using the Alk / Std method. A standard curve is also constructed using this method.

Table 8. Ingredients used for making mayonnaise.

Ingredient The consignment A source Lipid Soluble Green Tea Extract (LSC) # 1301108643 Kemin food technologies Calcium Disodium EDTA # C060131 Premium Ingredients Intl, Carol Stream, IL FORTIUM ^® _brand R30 Unknown Kemin food technologies Soybean oil # 1402109973 Kemin RM 01320 Table salt not Mortons Pasteurized Frozen Egg Yolks (10% Salt) # 038V3-1 Oskaloosa Foods,
is free Ground mustard not Toneʹs ^® (ACH Food Companies) Distilled white vinegar
acidity 4.5-5.0% not Heinz ^® Water not Crystal Clear ^® bottled

Table 9. Recipe for mayonnaise per load.

Ingredient Target% Added mass Soybean oil 75.00 1125 ± 0.05 g Salt 0.61 9.18 ± 0.01 g Egg Yolk, 10% Salt 8.89 133.32 ± 0.05 g Ground mustard 1.00 15 ± 0.01 g Distilled White Heinz® Vinegar 12.60 189 ± 0.01 g Water 1.90 28.5 ± 0.01 g

Table 10. Chemicals used for PV / alkenale analysis.

Chemical Provider CAS # # Parties Bottled Hydroxytoluene (BHT) Acros organics 128-37-0 A0295070 Water (deionized, ultrafiltered) Fisher scientific 7732-18-5 133687 Xylenol Orange, Disodium Salt Fluka analytical 1611-35-4 BCBH9921V Isopropanol J.T. Baker 67-63-0 0000045208 Iron (II) ammonium sulfate hexahydrate Fisher scientific 7783-85-9 107682 Reagent A AlkaSafe Std MP Biomedicals Alk0214 Reagent B AlkaSafe Std MP Biomedicals Alk0214

Data analysis . This is an initial study aimed at screening for possible natural A / O that can replace EDTA. For this reason, this time carry out only one experiment with each download. However, the time trend is studied for various types of processing, and it is used to compare samples with each other.

results

Comparison of oxidative products for various types of processing . Both PV and alkenals show that the untreated control appears to be the most oxidized sample for months 1-4 (Figure 1 and Figure 2). 500 ppm processed mayonnaise R30 appears to be less oxidized than the untreated control. However, there is still a higher amount of oxidative products than for the positive control with EDTA (75 ppm). However, with respect to PV, LSC at 250 ppm is as effective as EDTA (Figure 1), and for alkenals, the trend shows that it is more effective than EDTA (Figure 2), numerically.

Discussion

EDTA is a widely used synthetic chelating agent that acts as an antioxidant in mayonnaise. However, it, as a rule, is not considered favorable for this variety of product. Level 75 ppm chosen because it represents the highest permissible EDTA level in mayonnaise in the United States, and for this reason it represents the gold standard for controlling oxidation in mayonnaise.

After 4 months of storage under ambient conditions, the results of this study show that mayonnaise processed with 250 ppm LSC, is the least oxidized sample with characteristics comparable to those of EDTA. The PV values are very similar to EDTA throughout the studies, and the alkenals in the LSC sample are very similar to the EDTA sample for months 0-1, but real, they look slightly lower than for the EDTA sample for months 2-3. Obtained from natural sources of LSC at 250 ppm. represents an excellent alternative to EDTA.

EXAMPLE 3 - products from cereals and crushed grain

Despite the relatively low fat content, cereals and crushed grain ready-to-eat foods are still exposed to oxidative rancidity. The present study is the processing of extruded products from cereals or cereal grains using different combinations of ingredients and comparison to the untreated product (negative control), treated butylated gidroksiltoluolom (BHT) product (synthetic positive control) and treated FORTIUM ^® _brand MT70 (mixed tocopherols) Product (positive control obtained from natural sources). Samples are stored under accelerated conditions (40 ° C). The main factors affecting the shelf life of packaged cereals or crushed grains, and most importantly, their organoleptic attributes (aromatic and taste properties), are oxidative by-products (peroxide value -PV), volatile secondary oxidative by-products (hexanal). The accumulation of oxidation products is monitored instrumentally by examining peroxide numbers (PV) and the amount of hexanal. Changes in the organoleptic attributes of aromatic and flavoring properties are also tracked. Both chemical scores and organoleptic scores show some improvement over the untreated control when combinations of antioxidants, including peppermint extract (SE) and lipid-soluble catechins (LSC) are used, this shows that combinations of natural ingredients or ingredients derived from natural sources can be effective stabilizers for extruded cereal or crushed grain products.

Materials and methods

The starting materials used in the preparation of cereal or crushed grain products are shown in Table 11.

Table 11. Ingredients and recipe for extruded cereals and crushed grain

Target%
(from dry mix) Actually Added Weight (lbs (kg)) Ingredient Provider 60 350.0 (157.5) Whole Grain Flour 21st Century 35 204.2 (91.9) Native corn starch KPC 13700 four 23.3 (10.5) Granulated sugar United sugars corp one 5.8 (2.61) Fine scale salt Cargill not 135.0 g per load Canola oil, the party. # 1312111714 Kemin Animal Nutrition and Health (RM07794)

Products used to process cereal and crushed grain products are shown in Table 12.

Table 12. Types of processing used for extruded cereals and crushed grain

Antioxidant # Parties Provider # Product / RM The mass added to each load (g) FORTIUM ^® _brand MT70 1310109865 Kemin food technologies 016242 15.12 EN-HANCE ^® _brand BHT 1203101564 Kemin food technologies 01014 1.89 Verdilox ™ GT Liquid 1306103671 Kemin nutrisurance S016989 28.35 Spearmint Extract FORTRA ^® _brand 1402101496 Kemin food technologies 01680 9.92 FORTIUM ^® _brand MT95 Liquid 1307109107 Kemin food technologies 15515 4.25 ROSAN SF35 Liquid 1309100564 Kemin food technologies 015425 4.82

Processing levels are shown in Table 13. Two positive controls are used. These are BHT, which is a widely used synthetic antioxidant in extruded cereals and crushed grains, and mixed tocopherols, which are obtained from natural sources and are commonly used in cereals and crushed grains. The dosage of BHT is based on the upper allowable limit allowed for cereals and crushed grains. Dosage mixed tocopherols (FORTIUM ^® _brand MT70) is selected based on previous studies that showed that 400 ppm Mixed tocopherols, MT70, are effective in slowing down oxidation in extruded cereals and crushed grains. Verdilox GT Liquid (Kemin Industries, Inc., Des Moines, Iowa) is a potent drug effective in slowing the oxidation of fats in extruded pet granules. It is used in this study to evaluate its effectiveness in an extruded food product that is intended for human consumption. Lipid-soluble catechins (LSC) are an esterified form of water-soluble catechins, and, as shown, they are effective in slowing down oxidation in fats and oils. They are one of the components in Verdilox GT Liquid. Peppermint Extract (SE) is a water soluble ingredient that has been shown to be effective in slowing the oxidation of milk fat in liquid and powdered milk. Recipe for tocopherols + SE + rosemary extract (TRS) taken from previous studies of milk fat stabilization.

Table 13. Processing levels (ppm) of extruded cereal and crushed grain products. SE = peppermint extract.

Code MT70 Verdilox GT Rosan SF35 MT95 SE Bht Uht MT70 400,0 Verdilox 750.0 Verdilox + SE 750.0 40,0 TRS 127.5 112.5 40,0 Bht 50,0

Ways.Generally 12 loads (45 pounds (10 kg) each) of cereal and crushed grain products are extruded at the University of Nebraska-Lincoln pilot plant. Prepare two downloads (n = 2) for each treatment group. Products from cereals and crushed grain are prepared using a Wengert TX-57 twin-screw extruder (Wengert Manufacturing, Sabetha, KS). The dry mix is kneaded in the form of a large masterbatch, then divided / distributed into 45 lb (10 kg) downloads. All preparations (except SE) are mixed in 135 grams of oil. Four pounds (1.8 kg) of the dry mixture is removed from each 45 pound (10 kg) charge, oil is added, and manual mixing is performed until a homogeneous mixture is obtained. This mixture is added back to the remaining dry mixture and stirring is carried out for 10 minutes using a blender. The SEs are dry blended in 1 lb (0.45 kg) dry mix, which is then combined with the rest of the dry mix. The extrusion of each sample lasts 17 minutes, including 9 minutes of cleaning with passing pure material. The cereal and crushed grain product that is extruded during the cleaning period is not collected in order to minimize cross-contamination of various loads. After extrusion, the samples are packed ~ 100 g in each bag for cereals and crushed grains from low density polyethylene (LDPE) and are thermally sealed. One sample of each species is transported back to the laboratory to be analyzed the next day, and the remaining bags (24 in each group) are sent in a few days.

Samples are evaluated every 10 days for 155 days. On day 50, the frequency of studies is reassessed and changes up to once every 2-3 weeks due to such considerations that the content of oxidative by-products remains low in the first part of the study. At each point in time, one bag is opened from each load for sensory and instrumental analysis. Moments for the study of stored products from cereals and crushed grain represent day 1 under environmental conditions (ʺ day 0 ʺ on the graphs) and days 9, 20, 30, 40, 50, 71, 92, 113, 134, 155.

Analysis of peroxide numbers and hexanals. Products from cereals and crushed grains are analyzed for primary oxidation products (PV) and secondary oxidation products (hexanal). Hexanals are selected because they, as shown, are a good parameter that has a positive correlation with organoleptic changes in extruded cereals and crushed grains. Hexanal is determined in situ using GC analysis following established procedures.

Data analysis . Comparison of the content of carnosic acid and pH values for all samples is carried out using Analysis of Variance (ANOVA) using the software package STATGRAPHICS Centurion XV.

Organoleptic analysis . Sensory evaluation is carried out on several copies of samples of products from cereals and crushed grain. Organoleptic evaluators attend 2-30-minute training sessions to familiarize them with the 2 attributes in question (oxidized aroma and oxidized taste). One ounce plastic sample cups (28 g) (Daily Chef, Bentonville AR) are filled about 1/2 of their volume with cereals and crushed grains and sealed with plastic lids. For training, experts are provided with examples labeled as absent, medium, or very oxidized taste and aroma. They were asked to rate samples on a 15 cm scale, where absent = 0 and 15 = extremely strong. A mark on the linear scale represents the perceived attribute intensity. Experts are instructed on an appropriate assessment procedure for both taste and aroma. The aroma is evaluated first with the help of experts instructed to shake the sealed sample, then slightly open the sample and smell it. A napkin of plain white paper is served, and experts are instructed to sniff this napkin between samples to remove their aroma from their nostrils. Taste assessment experts are instructed to taste the sample, determine the grade, and then take a sip of water and bite off a piece of unsalted cracker between the samples. After discussion in a group of samples, experts supply blindly labeled samples from the same examples and ask them to rate the samples, with the goal of obtaining ratings similar to labeled samples. For storage studies for organoleptic evaluations, 3-digit random codes are labeled. The cups are filled with approximately 1 gram of cereal and crushed grain products and sealed with lids. Experts are supplied with a labeled sample, which is considered the average standard for both oxidized taste and oxidized odor. Experts are instructed to evaluate samples using the procedure used during training sessions.

results

PV results are shown in FIG. 3. Data differences between treatments are not visible until later storage times. The PV value in cereals and crushed grains processed by FORTIUM® _brand MT70 is maintained increasing, and in the end, it is numerically higher than for other types of processing. However, the PV value for other types of processing, with the exception of Veridlox, reaches a peak and decreases closer to the end of the storage time with acceleration. For example, for BHT treatment, it rises to 113, then experiencing a significant drop.

According to Figure 4, the content of hexanal begins to accumulate after day 70 of storage time. With the exception of day 113, unprocessed cereal and crushed grain products have a numerically higher hexanal content than for other types of processing until day 155, at which point the hexanal content begins to decrease. The hexanal content of cereals and crushed grain products treated with BHT begins to increase after day 70 and begins to decrease after day 113. The combination of mixed tocopherols, peppermint extract and rosemary extract (TRS) is still effective in maintaining a lower hexanal content compared to with raw control. Verdilox GT, Verdilox GT + peppermint extract and MT70 give the lowest amount of hexanal until day 134. And it can be seen that adding peppermint extract to Verdilox GT (Verdilox + SE) does not give an additional benefit while maintaining a lower hexanal content compared to processing only Verdilox GT.

The organoleptic properties assessment results are shown in Tables 15 and 16. A larger number indicates a higher intensity of oxidized taste or aroma. Estimates of oxidized aroma show significant differences between treatments on days 10, 40, 70, 113, 134 and 155. At the end of the study period (day 155), there was a statistically significant difference ( p <0.05) between unprocessed cereal and crushed grain and cereal and crushed grain products processed by BHT. Estimates for oxidized taste show statistically significant differences between treatments on days 92-155. On day 113, MT70, Verdilox and TRS give significantly lower oxidized taste ratings than for untreated samples or for samples treated with BHT. On day 134, all samples had significantly lower oxidized taste ratings than for the untreated sample. By day 155, differences between treatments are becoming less apparent.

Table 15. Estimates for oxidized aroma, for cereals and crushed grains under storage conditions with acceleration (40 ° C). The values in the column with different superscripts are statistically significantly different ( p <0.05)

Accelerated Storage Days 0 ten 20 thirty 40 50 70 92 113 134 155 Raw 1,62 1.96 ^b 2.24 1.77 1.89 ^s 2,33 4.44 ^b 4.93 4.08 ^cd 4.96 ^b 3.72 ^b Bht 1,04 1.31 ^ab 1.88 1.24 1.65 ^bc 1,64 1.88 ^ab 4.71 5.51 ^d 2.22 ^a 2.02 ^a MT70 1.21 1.64 ^b 2.09 1.34 1.32 ^ab 1.28 1.46 ^ab 1,63 1.97 ^a 3.07 ^a 2.73 ^ab Verdilox + SE 1.42 1.76 ^b 1.68 1.30 1,03 ^a 1.19 1.69 ^ab 1.68 3.81 ^bcd 3,55 ^ab 3.81 ^ab Verdilox 1.65 1.53 ^ab 1,64 1.37 1,60 ^ab 1,59 1.42 ^ab 1.97 2.41 ^abc 3.29 ^ab 4.13 ^ab TRS 1.48 0.88 ^a 1.68 1.37 1.47 ^b 1.17 1.18 ^a 1.32 2.23 ^ab 3.5 ^9ab 3.01 ^ab

Table 16. Estimates for the oxidized taste for cereals and crushed grains under storage conditions with acceleration (40 ° C). The values in the column with different superscripts are statistically significantly different ( p <0.05)

Accelerated Storage Days 0 ten 20 thirty 40 50 70 92 113 134 155 Raw 1.35 1.22 1.77 1,54 1.55 2.02 3.11 4,56 ^b 4.03 ^b 6.67 ^b 4.82 ^b Bht 0.96 1.96 1.90 1.36 1,53 1.41 1.36 3.28 ^ab 4.32 ^b 2.06 ^a 1.90 ^a MT70 1.40 2.23 1.73 1,57 1.26 1.16 1,54 1,40 ^a 2.10 ^a 2.17 ^a 2.81 ^ab Verdilox + SE 1,50 1.42 2.04 1,57 1.12 1.23 1,50 1.29 ^a 3.34 ^ab 2.31 ^a 3.89 ^ab Verdilox 1,67 1.55 1.81 1.81 1.49 1.34 1.72 1.14 ^a 1.99 ^a 2.45 ^a 3.68 ^ab TRS 0.94 1,63 1.46 1.70 1,69 1.21 1.35 1.18 ^a 1.81 ^a 3.56 ^a 3.29 ^ab

Discussion

The values for PV, hexanal, oxidized aroma and oxidized taste all correlate for samples treated with BHT from day 113 to day 155, reaching the highest concentration on day 113 and falling on day 134 and 155. It is possible that on day 113, PV accumulation in BHT-treated cereals and crushed grains and unprocessed cereals and crushed grains reaches a peak, and peroxide decomposition begins to dominate. The decomposition of peroxides produces secondary oxidation products, which have a direct correlation with changes in the taste and smell of cereals and crushed grains. The content of hexanals between 5 and 10 ppm, as shown, correlates with the oxidized aroma in low-fat dry foods. The hexanal content begins to rise after day 113, at which point the scores of the oxidized aroma also increase. For most samples, hexanal does not begin to form until the days between days 70 and 92. It is possible that at this time, additional oxidation begins to dominate, which consumes some of the unstable hexanal. The pattern of changes in hexanal content is very different for samples with BHT from all other types of processing, so it is possible that the oxidation path in samples treated with BHT is different.

EXAMPLE 4 - Effects of antioxidants on the oxidative stability of margarine at elevated storage temperature

Margarine with a fat content of approximately 80% is processed using various natural or synthetic ingredients to study antioxidant effects. Lipid-soluble green tea extract (LSC) is the best at obtaining the smallest amount of oxidative products during the storage time of margarine. It could be used as a natural alternative to the synthetic antioxidant BHA / BHT in margarine.

Materials and methods

Materials and chemicals . EN-HANCE ^® _brand BHA dry, EN-HANCE ^® _brand BHT dry, FORTIUM ^® _brand MT90, lipid-soluble green tea (LSC or EN-FORT ^™ 101 dry), FORTIUM ^® _brand R20 (rosemary extract / sunflower oil), FORTIUM ^® _brand R40 (rosemary extract / sunflower oil), ascorbic acid (VC) and sodium caseinate (SC) are available from Kemin Food Technologies (Zhuhai, China). Crude oil (melting point 38-42 ° C), supplied by Wilmar (Qihuangdao, China), contains palm oil, soybean oil, an unknown emulsifier, flavor and pigment in an unknown relationship. The resulting margarine consists of 84% crude oil and 16% distilled water.

Xylenol orange, disodium salt (indicator quality), iron (II) ammonium sulfate hexahydrate (AR, 99.5%), p-anisidine (99%), sulfuric acid (98%), glacial acetic acid (99.5%) , hydrogen peroxide (AR, 30% in water), isopropanol (quality for HPLC, 99.8%), isooctane (quality for HPLC, 99.0%) are purchased from Aladdin Reagents Inc. (Shanghai, China).

Sample preparation . The crude oil is completely melted at 60 ° C in a water bath and processed with the following ingredients, individually: (1) this is an untreated control, (2) 84 ppm. EN-HANCE BHA + 84 ppm EN-HANCE BHT (positive control 1), (3) 100 ppm FORTIUM ^® _brand MT90 (mixed tocopherols) (positive control 2), (4) 125 ppm LSC (LSGT), (5) 250 ppm LSC, (6) 500 ppm. FORTIUM ^® _brand R20, (7) 1000 ppm FORTIUM ^® _brand R20, (8) 200 ppm VC + 250 ppm FORTIUM ^® _brand R40, (9) 200 ppm VC + 250 ppm FORTIUM ^® _brand R40 + 50 ppm SC. Application fractions are given in relation to the total weight of margarine (Processing 3-9) and to the total fat content in margarine (Processing 2). All types of processing are carried out once.

Margarine is emulsified by pouring heated distilled water (60 ° C) into crude oil, and the mixture is homogenized in a high speed blender for 30 minutes. The homogenized mixture is kept in a freezer at -18 ° C and manually stirred from time to time until it is cured (about 30-40 minutes). Each treatment product is divided into 6 servings. Each portion was placed in a 50 ml transparent polyethylene conical centrifuge tube (Fisher Scientific Pte Ltd, China) and stored in an oven without exposure to light at 35 ° C for 6 weeks storage study. At each moment of the study, 2 servings of 5-gram samples are taken from one 50-ml test tube for analysis, for each type of treatment.

Chemical analyzes . Peroxide numbers (PV, initial oxidative by-products) in margarine are measured using the FOX II method (oxidation of iron (II) in xylenol orange) (000-KNCLSM-017) on a Shimadzu UV-2401PC spectrophotometer. p-Anisidine numbers are measured in accordance with AOCS Official Methods Cd 18-90 (050KFTWW-M.062). The absorption coefficient at 350 nm was measured (A _b ) on the same Shimadzu UV-2401PC spectrophotometer using isooctane as the background. Each measurement is carried out twice.

Data analysis . Multiple regression analyzes for peroxide numbers and p-anisidine numbers among various treatments are performed using the STATGRAPHICS ^® Centurion XV software package.

results

PV values in untreated margarine and margarine, processed FORTIUM ^® _brand MT90, rapidly increased during the storage at 35 ° C (Figure 5). FORTIUM ^® _brand MT90 and untreated controls give similar peroxide numbers. All other types of processing can slow down the accumulation of peroxides, the content of which remains below the threshold level (10 meq / kg of fat) during the storage period. Typically, a food product is believed to have rancidity problems if PV is above a threshold level.

LSC at 250 ppm and two drugs for treatment which comprise FORTIUM ^® _brand R40, exceed the characteristics of the combination EN-HANCE BHA and EN-HANCE BHT (positive control 1) (5). LSC at 125 ppm and FORTIUM ^® _brand R20 at two dosage levels works similarly to positive control 1. From 50 ppm. SC or without two drugs for treating containing VC and FORTIUM ^® _brand R40, provide similar peroxide numbers throughout the storage period.

p- Anisidine numbers also increase during the storage period for all types of processing (Figure 6). Comparison of the steepness and intersection of individual regression lines shows that processing LSC, FORTIUM ^® _brand R20 and VC + FORTIUM ^® _brand R40 gives lower p-anisidine numbers than for untreated samples. Anisidine numbers during EN-HANCE BHA + EN-HANCE BHT processing (positive control 1) are also lower than for untreated samples. FORTIUM ^® _brand MT90 at 100 ppm not effective in lowering p-anisidine numbers compared to untreated samples.

Processing with 125 and 250 ppm LSC, 1000 ppm FORTIUM ^® _brand R20 and 200 ppm VC + 250 ppm R40 + 50 ppm SC works better than FORTIUM ^® _brand MT90. Processing with 500 ppm FORTIUM ^® _brand R20 and 200 ppm VC + 250 ppm R40 gives lower anisidine numbers than for a sample treated with 100 ppm. FORTIUM ^® _brand MT90.

Compared to 84 ppm, EN-HANCE BHA + 84 ppm EN-HANCE BHT, LSC has better performance when it is dosed at 125 ppm. It has significantly higher efficiency while maintaining lower anisidine numbers when the dosage rises to 250 ppm. At the same time, processing 200 m .d. VC + 250 ppm R40 + 50 ppm SC gives a trend that supports a lower anisidine number compared to BHA + BHT treatment. C 50 ppm SC or without it, there is no difference in performance between the two preparations for processing, which contain 200 ppm VC + 250 ppm R40.

Discussion

This study identifies the ability of several ingredients to protect margarine from lipid oxidation. There is a clear trend during storage time. Processing LSC (125 and 250 ppm), processing 1000 ppm FORTIUM ^® _brand R20 and VC + treatment. FORTIUM ^® _brand R40 can slow down the accumulation of primary and secondary oxidative by-products in margarine, as shown by peroxide and p-anisidine numbers. In addition, the positive control, FORTIUM ^® _brand MT90, shows great effectiveness in protecting against oxidative rancidity margarine, although mixed tocopherols are widely used in the margarine industry. Another positive control, the combination of EN-HANCE BHA + EN-HANCE BHT, could protect the margarine effectively at a significantly lower peroxide number and at a numerically lower anisidine number than for the untreated sample.

Compared to FORTIUM ^® _brand MT90, processing is both 125 and 250 ppm. LSC, 1000 ppm FORTIUM ^® _brand R20 and 200 ppm VC + 250 ppm R40 + 50 ppm SC has shown significant efficacy in protecting the oxidative stability of margarine. LSC at 250 ppm works better than 84 ppm EN-HANCE BHA + 84 ppm EN-HANCE BHT at a lower level of primary and secondary oxidative products. Sodium Caseinate (SC) is a milk protein and is widely used as a metal chelating agent that can potentially chelate a heavy metal catalyst for lipid oxidation. In the present study, with 50 ppm SC or without it, there is no difference between the two treatment preparations containing 200 ppm VC + 250 ppm FORTIUM ^® _brand R40,

Since both BHA and BHT are synthetic chemicals, LSC, a natural product ingredient, can serve as an alternative ingredient for combining BHA + BHT while maintaining the oxidative stability of margarine. In addition to this, the present study shows that LSC / rosemary extract supports oxidative stability better than mixed tocopherols for margarine, and for this reason can act as a solution, as a substitute for tocopherols in margarine.

EXAMPLE 5 - Oxidative stability of a farm salad dressing under the influence of various types of processing

Due to its high fat content, farm salad dressings are sensitive to lipid oxidation, which reduces the shelf life of packaged foods. Volatile compounds, which are formed from secondary oxidative by-products, contribute to the quality of taste and to the disappearance of tastes and smells. Ethylene diamine tetraacetate (EDTA) is typically used to slow oxidation in farm salad dressing because it is inexpensive and highly effective at a maximum authorized dose of 75 ppm. However, there is an increasing consumer demand for natural products and many companies are interested in natural alternatives. for EDTA. The purpose of this study is to compare Kemin Food Technologies (KFT) GT- FORT ™ 101 (lipid soluble green tea / sunflower _{^{oil) (GTF), FORTIUM ® brand}} R30 ( rosemary extract) (R30), and combinations thereof during deceleration occurrence of oxidative rancidity for farming refueling for the salad.

Materials and methods

Materials The materials used in preparing salad dressings are shown in Tables 17 and 18. GT-FORT 101 SF and R30 are obtained from KFT Customer Laboratory Services (CLS). EDTA is obtained from Premium Ingredients (Carol Stream, IL).

Table 17. The starting materials used in the preparation of farm salad dressings

Ingredient Percent Provider Location Soybean oil 56.00 * KANA Des Moines, IA Water 25.89 Crystal clear Des Moines, IA Farm dressing for salad dressing 8.71 Elite spice Jessup, MD White vinegar (diluted to 120 grains) 5.90 * KANA Des Moines, IA Egg Yolk (10% Salt) 3,50 Oskaloosa egg Oskaloosa, IA Potassium sorbate 0,025 Prinova Carol Stream, IL

* Kemin Animal Nutrition and Health

Table 18. The level of inclusion of preparations for processing in the farm salad dressing (ppm).

Dosages refer to the total weight of the dressing.

# Processing GT-FORT 101 SF
(20140716-01) R30 (20140703-01) EDTA (C060131) one - - - 2 75 (0.3 g) 3 1250 four 600 five 600 6 600 100 7 600 250 eight 600 400 9 600 600 ten 800 250 eleven 1000 250 12 1250 250

Mixing Instructions. A farm salad dressing is prepared using a KitchenAid ^® mixer (325 watts, St. Joseph, MI) with a paddle. For each of the 12 downloads, 400 grams are prepared. The eggs are weighed in a stainless steel cup and beat at low setting (# 2) for 30 seconds. The mixer is stopped and the side walls of the cup are cleaned with a rubber spatula to incorporate the entire mixture from the side walls of the cup. Beat the mixture for an additional 30 seconds at speed # 2. Potassium sorbate is dissolved in water, which is then added and stirred for 30 seconds at speed # 2, the cup is cleaned, and stirring is performed for an additional 30 seconds at speed # 4.

Oil is added very slowly over 5 minutes, at which time the mixer mixes at speed # 4. After adding the oil, add vinegar for 30 seconds, at which time the mixer mixes at speed # 4. The mixer is stopped and seasoning is added for the farm salad dressing in one portion, and then stirring is carried out for 30 seconds at a speed of # 4. The mixture is then transferred to a food processor (Black and Decker, USA) and mixed for 30 seconds.

Storage conditions . Samples are packaged in separate 2 oz. (56 g) PET bottles (Fisher Scientific item 02991683) to allow different samples to open during each study period. Samples are stored at test temperature with acceleration (40 ° C).

Stability analysis . Samples are analyzed for alkenals (secondary oxidative by-products) and peroxide numbers (PV).

results

The results of the study of oxidative by-products are shown in Figures 7 and 8. The obvious difference in the data starts from week 6. The untreated sample has the highest PV value starting from week 2 and the alkenale content starting from week 6. The alkenale content is the lowest for GTF / R30 600/400 and 600/600 per week 10. Samples treated with EDTA generally give the second highest levels of alkenals. The addition of either rosemary or GTF, or a combination thereof, results in lower alkenale levels. All combinations result in lower levels of alkenals.

For PV, the data differences for each type of treatment become more pronounced closer to the final stages of research. Combined samples with GTF / R30 600/250, 600/400 and 600/600 have the lowest PV values per week 10. The extreme value or tolerance limit for soybean oil (used in this matrix) is 10 meq / kg of fat. By week 10, all samples are above this limit.

For a combination of both PV and alkenals, a treatment of 600 ppm GTF combined with various levels of rosemary results in the lowest oxidative content in this farm salad dressing.

EXAMPLE 6 - Emulsifying properties of the LSC at the interface.

Materials and methods

Materials Sorbitan monooleate (span 80), triglycerol dioleate (TGDO), lipid-soluble green tea (LSC, lot # 1401101795, Kemin Bioscience, Ningbo, China), sodium chloride (99.5%), ultrapure water, soybean oil (purchased at a local supermarket). Span 80, TGDO and sodium chloride are purchased from Aladdin Reagent, Shanghai, China.

Stability study of LSC-treated soybean oil / water emulsions. The stability of soybean oil / water emulsions is evaluated by measuring the time variation of the volume fraction of the emulsion phase at 25 ° C. An oil-in-water emulsifier like Span 80, TGDO or LSC (0.50 g) is first dissolved in 50 ml of soybean oil in a 250 ml beaker. It is necessary to heat soybean oil to 80-90 ° C to facilitate the dissolution of LSC. Then add a portion of 50 ml of saline (15% by weight of sodium chloride in ultrapure water). The biphasic solution is homogenized at 17500 rpm for 2 minutes using an IKA Ultra Turrax T25 basic homogenizer. Then, the resulting emulsion is immediately transferred to a 100 ml graduated cylinder. Then the emulsion begins to separate, with the emulsion phase above and the aqueous phase below. The volume of the emulsion phase is recorded after 5 minutes, 10 minutes, 30 minutes, 60 minutes and 24 hours of separation. Each treatment (span 80, TGDO, LSC and without treatment) is carried out three times. The volume fraction of the emulsion phase is calculated by dividing the volume of the emulsion phase (ml) by the total volume of water and oil (100 ml).

Improving the stability of food emulsion. W apravku dressings and mayonnaise are prepared according to the recipe of Table 19 and Table 20.

Farm salad dressing is mixed using a KitchenAid ^® mixer with paddle attachment. The eggs are weighed in a stainless steel cup and beat at low setting (# 2) for 30 seconds. The side walls of the cup are cleaned and the eggs are beaten for another 30 seconds. Water is added and then stirred for 30 seconds, the cup is cleaned, and then stirring is continued for an additional 30 seconds when setting speed # 4. When setting speed # 4, oil is added very slowly. After adding oil, add vinegar for 30 seconds when setting speed # 4. Then add the seasoning mixture for the farm salad dressing and stirring for 30 seconds when setting the speed # 4. The mixture is transferred to a food processor and mixed for 30 seconds.

To make mayonnaise, egg yolks are first beaten in a KitchenAid ^® (Heavy Duty) mixer using a wire whisk for 30 seconds with speed setting # 2. Then add salt and mustard and mix for an additional 30 seconds while setting speed # 4, cleaning the side walls with a spoon 3 times. Then water is added and stirring is performed for 30 seconds when setting speed # 2, then the cup is cleaned, then stirring is continued for an additional 30 seconds when setting speed # 4. Then they add oil very slowly at speed setting # 4, in small portions (especially at the beginning, when they add only a few ml and allow them to be absorbed in the eggs before adding more). For this amount of mayonnaise, it takes approximately 15 minutes of total time to add oil. Toward the end, the oil is added in a thin stream. After adding all the oil, add vinegar for 30 seconds when setting speed # 2. Then it is mixed for an additional 30 seconds, alternately at speed settings # 2 and # 4. The total mixing time is 5-10 minutes.

The salad dressing and mayonnaise are frozen at -20 ° C overnight and thawed in a water bath at 60 ° C for 1 hour.

Table 19. Recipe for farm salad dressing.

Component Number Material % RM01320 Soybean oil 56.00 Crystal Clear® Water 25.89 Elite Spice 31017A9 Version 1 Farm dressing for salad dressing 8.71 RM16833 White vinegar (diluted to 120 grains) 5.90 Oskaloosa egg Egg Yolk (10% Salt) 3,50

Table 20. Recipe for mayonnaise per load.

Ingredient Target% Added mass Soybean oil
Salt
Egg Yolk, 10% Salt
Ground mustard
Distilled White Heinz® Vinegar 75.00
0.61
8.89
1.00
12.60 1125 ± 0.05 g
9.18 ± 0.01 g
133.32 ± 0.05 g
15 ± 0.01 g
189 ± 0.01 g Water 1.90 28.5 ± 0.01 g

results

Comparison with other emulsifiers . The graph of the volume fraction of the emulsion depending on the separation time is shown in Fig.9. It shows that within 10 minutes of separation, the phase volume of the emulsion with HGDO and LSC treatment decreases more slowly than without treatment. However, after 10 minutes of separation, only the LSC-treated emulsion retains a consistently higher emulsion volume (64%) while the emulsion volume for all other treatments drops to 55% at a 60-minute separation time. The volume fraction of the emulsion phase after this remains unchanged for all types of processing even after 24 hours. These results show that LSC helps stabilize the oil-in-water emulsion and that LSC has better emulsification properties than the two commonly used oil-in-water emulsifiers - span 80 and HGDO - in soybean oil / water emulsions.

Emulsion stability in food emulsion. For both food emulsions, for processed farm salad dressing and for mayonnaise, LSC-treated samples are physically more stable, leaving only one phase after repeated freezing and thawing cycles, which usually break the emulsion and result in two phases (water phases and oil).

The above description and drawings include illustrative embodiments of the present invention. The above-described embodiments and methods described in the present invention may vary based on the ability, experience and preferences of a person skilled in the art. By itself, the enumeration of the stages of the method in a certain order does not impose any restrictions on the order of implementation of the stages of the method. The above description and drawings only explain and illustrate the present invention, and the present invention is not limited thereto, unless the claims are so limited. Those skilled in the art who have a description in front of themselves can make modifications and changes therein without departing from the scope of the present invention.

Claims (10)

1. A method of slowing down the oxidation of food products having a lipid-water phase interface, characterized in that it comprises the step of adding green tea catechins esterified to palmityl esters in an amount of 250-1000 ppm, green tea catechins esterified to palmityl esters, they are introduced into the food product together with antioxidant compounds by stirring, and these food products are selected from the group consisting of food emulsions, meat products, as well as products from cereals and from crushed grains with a low fat content, while food emulsions are selected from the group consisting of mayonnaise, margarine and salad dressings. 2. The method according to claim 1, in which the food product is meat and the method results in slowing down unwanted color changes of the meat. 3. The method according to claim 1, in which the food product is meat and the method prolongs the oxidative stability of meat. 4. The method according to claim 1, in which the food product is selected from the group consisting of fats and oils. 5. The method according to claim 4, in which the oil is selected from the group consisting of vegetable oils. 6. The method according to claim 1, in which the food product is selected from the group consisting of extruded food products. 7. The method according to claim 1, in which the effective amount is in the range between 10 ppm and 5000 ppm mass from a food product. 8. The method according to claim 7, in which the effective amount is in the range between 100 ppm. and 1000 ppm 9. The method according to claim 1, further comprising adding an antioxidant compound to the food product. 10. The method according to claim 9, in which the antioxidant compound is selected from the group consisting of BHA, BHT, tert-butylhydroquinone, gallates, ascorbic acid, erythorbic acid, ascorbyl palmitate, tocopherols, tocotrienols, carotenoids, anthocyanins, polyphenols, citric acid, , EDTA, glycine, lecithin, polyphosphates, tartaric acid, trihydroxybutyrophenone, thiodipropionic acid and dilauryl and distearyl esters.

Images